Triethylamine → 4D-083

HRID 1995344노트

반응식

HRID 1995344 반응식
[O:1]=[C:2]1[C:7]([C:8](O)=[O:9])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1.C([N:19](CC)CC)C.S(Cl)(Cl)=O>O1CCCC1>[O:1]=[C:2]1[C:7]([C:8]([NH2:19])=[O:9])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 121489343-Oxo-6-phenyl-2,3-dihydropyridazine-4-carboxylic acid

생성물 1

HCID 14753284D-083

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In an alternate procedure, a mixture of 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxylic acid (1.92 g), triethylamine (3.0 ml), and thionyl chloride (5.0 ml) in tetrahydrofuran is allowed to stir at 20°-25° C. for 6 hours. The mixture is concentrated on the rotary evaporator and the residue is treated with 50 ml of cold ammonium hydroxide solution. The solid product is collected and recrystallized from acetic acid to give 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxamide.

후처리

  1. concentrationThe mixture is concentrated on the rotary evaporator
  2. additionthe residue is treated with 50 ml of cold ammonium hydroxide solution
  3. customThe solid product is collected
  4. customrecrystallized from acetic acid

출처 및 근거

ORD 기록
ord-091ee31fa94a4af29767edc1a3780f19
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04404203

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